JP2014088516A - スクリーン印刷用導電性接着剤並びに無機素材の接合体及びその製造方法 - Google Patents
スクリーン印刷用導電性接着剤並びに無機素材の接合体及びその製造方法 Download PDFInfo
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- JP2014088516A JP2014088516A JP2012239957A JP2012239957A JP2014088516A JP 2014088516 A JP2014088516 A JP 2014088516A JP 2012239957 A JP2012239957 A JP 2012239957A JP 2012239957 A JP2012239957 A JP 2012239957A JP 2014088516 A JP2014088516 A JP 2014088516A
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- Prior art keywords
- metal
- conductive adhesive
- screen printing
- viscosity modifier
- inorganic material
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
- H05K3/321—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J177/00—Adhesives based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Adhesives based on derivatives of such polymers
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
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Abstract
【解決手段】金属ナノ粒子(A1)及びカルボキシル基を有する保護コロイド(A2)を含む金属コロイド粒子(A)と、アミド結合及び/又は尿素結合粘度調整剤(B)と、分散溶媒(C)とを組み合わせて、スクリーン印刷用導電性接着剤を調製する。前記粘度調整剤(B)はウレア変性ポリアミド骨格を有していてもよい。前記粘度調整剤(B)は、さらにポリオキシC2−4アルキレン基及び/又はアルキル基を有していてもよい。前記分散溶媒(C)は、大気圧下における沸点が240〜300℃のアルコール類であってもよい。
【選択図】なし
Description
本発明のスクリーン印刷用導電性接着剤は、金属ナノ粒子及びカルボキシル基を有する保護コロイドを含む金属コロイド粒子(A)と、アミド結合及び/又は尿素結合を有する粘度調整剤(B)と、分散溶媒(C)とを含む。
金属コロイド粒子(A)は、金属ナノ粒子(A1)と、カルボキシル基を有する保護コロイド(A2)とを含んでいればよく、金属ナノ粒子(A1)と保護コロイド(A2)とは独立して存在していてもよいが、金属ナノ粒子の(A1)の分散性を向上できる点から、金属ナノ粒子(A1)と、この金属ナノ粒子(A1)を被覆する保護コロイド(A2)で構成された金属コロイド粒子であってもよい。
金属ナノ粒子(A1)を構成する金属(金属原子)としては、例えば、遷移金属(例えば、チタン、ジルコニウムなどの周期表第4A族金属;バナジウム、ニオブなどの周期表第5A族金属;モリブデン、タングステンなどの周期表第6A族金属;マンガンなどの周期表第7A族金属;鉄、ニッケル、コバルト、ルテニウム、ロジウム、パラジウム、レニウム、イリジウム、白金などの周期表第8族金属;銅、銀、金などの周期表第1B族金属など)、周期表第2B族金属(例えば、亜鉛、カドミウムなど)、周期表第3B族金属(例えば、アルミニウム、ガリウム、インジウムなど)、周期表第4B族金属(例えば、ゲルマニウム、スズ、鉛など)、周期表第5B族金属(例えば、アンチモン、ビスマスなど)などが挙げられる。金属は、周期表第8族金属(鉄、ニッケル、ロジウム、パラジウム、白金など)、周期表第1B族金属(銅、銀、金など)、周期表第3B族金属(アルミニウムなど)及び周期表第4B族金属(スズなど)などであってもよい。なお、金属(金属原子)は、保護コロイドに対する配位性の高い金属、例えば、周期表第8族金属、周期表第1B族金属などである場合が多い。
保護コロイド(A2)は、カルボキシル基を有する有機化合物(カルボキシ有機化合物)と、高分子分散剤とで構成されている。
粘度調整剤(粘稠剤又はレオロジーコントロール剤)(B)は、接着剤中で保護コロイドに含まれるカルボキシル基と水素結合可能な添加剤であり、カルボキシル基と水素結合可能であるために、分子内に水素原子と陰性原子(酸素原子及び窒素原子)とを有しており、水素結合の結合強度が大きく、増粘性や溶媒との相溶性も高い点から、アミド結合及び/又は尿素結合(特にアミド結合)を有している。そのため、アミド結合及び/又は尿素結合は保護コロイドと相互作用することで、少ない添加量でもペースト状の接着剤の粘度を大幅に改善可能であり、スクリーン印刷性を向上できる。また、このような水素結合を発現する粘度調整剤の場合、接着剤の硬化時に、被接着面に粘度調整剤が溜まり難く、金属接合を阻害し難い。
分散溶媒としては、前記金属ナノ粒子(又は金属コロイド粒子)を接着剤中で分散できればよいが、スクリーン印刷性の点から、大気圧下における沸点が220℃以上の溶媒が好ましい。分散溶媒の大気圧下における沸点は、例えば、220〜300℃、好ましくは230〜280℃、さらに好ましくは240〜270℃程度である。分散溶媒の沸点が低すぎると、導電性接着剤をスクリーン印刷で塗布し、例えば、厚み5〜20μm、巾30〜100μm程度のパターンを形成させた場合、乾燥が激しく、チップ実装マウントを行うまでに溶剤が乾燥してしまい、接着不良となり易い。一方、沸点が高すぎると、導電性接着剤の硬化条件下(通常100〜300℃、3〜120分間)で溶媒が揮発し難く、接着層に損損し易く、硬化温度の高温化又は硬化時間の長時間化を行う必要があり、半導体チップの劣化又は生産性の低下を招き易い。
本発明のスクリーン印刷用導電性接着剤は、無機素材を接合するために用いられる。詳しくは、無機素材の接合体は、第1の無機素材に前記導電性接着剤をスクリーン印刷する印刷工程、第2の無機素材で前記導電性接着剤を挟み込んだ後、100℃以上で加熱して前記導電性接着剤を焼結する焼結工程を経て得られる。すなわち、本発明の無機素材の接合体は、第1の無機素材と第2の無機素材との間に、前記導電性接着剤を介在させて、前記導電性接着剤を焼結することにより得られる。
(銀コロイド粒子調製)
硝酸銀66.8g、酢酸(和光純薬工業(株)製、沸点118℃)10g、カルボキシ基を有する高分子分散剤(COOH含有高分子)(ビックケミー・ジャパン(株)製「ディスパービック190」、酸価10mgKOH/g、有効成分40%、主溶剤:水)0.7gを、イオン交換水100gに投入し、激しく撹拌した。これに2−ジメチルアミノエタノール(和光純薬工業(株)製)100gを徐々に加えた。75℃で1.5時間撹拌後、球状銀粉が黒色沈殿物として生じた。デカンテーションによる上澄みの除去と水による希釈操作を繰り返し行い、初期の1000倍まで希釈した後、吸引ろ過により沈殿物を回収し、カルボキシ基含有保護コロイドで保護された銀ナノ粒子の湿潤ケーキ(銀コロイド粒子)を得た。
前記湿潤ケーキに溶媒として1,5−ペンタンジオール(和光純薬工業(株)製、沸点242℃)を加えた後、乳鉢で練りながら水を除去して、銀濃度88.0%の銀ナノ粒子分散ペーストを得た。
線径18μm、500メッシュ、乳剤厚み10μmのスクリーン版を用いて前記導電性接着剤を印刷し、L/S=50/50μmの櫛形パターンを形成し、以下の基準で評価した。
×:印刷後の線幅が前記基準を満たさない線幅である。
線径18μm、500メッシュ、乳剤厚み10μmのスクリーン版を用いて前記導電性接着剤を印刷し、基板上に500μm□(500μm×500μm)のパターンを形成させた。印刷後、室温下(25℃)で0、30、60、180、300分間放置した後、光学顕微鏡で印刷物が乾燥していないか確認した。具体的にはピンセットで印刷物を削り、乾燥物が剥離した場合を「×」と評価した。次いで、印刷された導電性接着剤パターンにチップをマウントし、せん断強度を確認した。また、印刷直後にチップマウントし、200℃、90分間硬化させたサンプルについては、せん断強度に加えて、破壊モードを観察し、凝集破壊(金属結合)、界面剥離(非金属結合)のいずれかであるか評価した。
導電性接着剤をスライドガラスにアプリケーターを用いて塗布し、200℃、90分間焼成して厚み3μmの導電膜を形成し、四探針法による表面抵抗と触針式膜厚計による膜厚から比抵抗を算出した。
実施例1で作製した銀ナノ粒子分散ペースト100部に、1,5−ペンタンジオール16.7部、粘度調整剤(BYK−431)4.4部を加え、温風ドライヤーを当てながら乳鉢で練り、粘度調整剤に含まれていたイソブタノール及びモノフェニルグリコールを除去して、銀濃度75%の導電性接着剤を得た。得られた導電性接着剤を実施例1と同様に評価した。
実施例1で作製した銀ナノ粒子分散ペースト100部に、1,5−ペンタンジオール9.7部、粘度調整剤(BYK−431)2.2部を加え、温風ドライヤーを当てながら乳鉢で練り、粘度調整剤に含まれていたイソブタノール及びモノフェニルグリコールを除去して、銀濃度80%の導電性接着剤を得た。得られた導電性接着剤を実施例1と同様に評価した。
実施例1で作製した銀ナノ粒子分散ペースト100部に、1,5−ペンタンジオール9.8部、粘度調整剤(BYK−431)1.1部を加え、温風ドライヤーを当てながら乳鉢で練り、粘度調整剤に含まれていたイソブタノール及びモノフェニルグリコールを除去して、銀濃度85%の導電性接着剤を得た。得られた導電性接着剤を実施例1と同様に評価した。
実施例1で作製した銀ナノ粒子分散ペースト100部に、1,5−ペンタンジオール33.4部、粘度調整剤(BYK−431)13.2部を加え、温風ドライヤーを当てながら乳鉢で練り、粘度調整剤に含まれていたイソブタノール及びモノフェニルグリコールを除去して、銀濃度65%の導電性接着剤を得た。得られた導電性接着剤を実施例1と同様に評価した。
実施例1で作製した銀ナノ粒子分散ペーストをそのまま使用し、実施例1と同様に評価した。
実施例1で作製した銀ナノ粒子分散ペーストに1,5−ペンタンジオールを加え銀濃度70%としたペーストを使用し、実施例1と同様に評価した。
溶媒をブチルカルビトールアセテートとしたこと以外は実施例1と同様にして作製した銀ナノ粒子分散ペースト100部に、ブチルカルビトールアセテート4.4部、増粘剤(日新化成(株)製「EC−200」、高分子量エチルセルロース、有効成分15%、主溶剤:ブチルカルビトールアセテート)5.6部を加え、乳鉢で練り、銀濃度80%の導電性接着剤を得た。得られた導電性接着剤を実施例1と同様に評価した。
溶媒をブチルカルビトールアセテートとしたこと以外は実施例1と同様にして作製した銀ナノ粒子分散ペースト100部に、ブチルカルビトールアセテート4.4部、増粘剤(EC−200)21.3部を加え、乳鉢で練り、銀濃度70%の導電性接着剤を得た。得られた導電性接着剤を実施例1と同様に評価した。
実施例1で作製した銀ナノ粒子分散ペースト100部に、1,5−ペンタンジオール22.2部、粘度調整剤としてカルボキシル基を有する高分子(ディスパービック190)5.5部を加え、温風ドライヤーを当てながら乳鉢で練り、粘度調整剤に含まれていた水を除去して、銀濃度70%の導電性接着剤を得たとしたこと以外は実施例1と同様に評価した。
Claims (9)
- 金属ナノ粒子(A1)及びカルボキシル基を有する保護コロイド(A2)を含む金属コロイド粒子(A)と、アミド結合及び/又は尿素結合を有する粘度調整剤(B)と、分散溶媒(C)とを含むスクリーン印刷用導電性接着剤。
- 粘度調整剤(B)がウレア変性ポリアミド骨格を有する請求項1記載のスクリーン印刷用導電性接着剤。
- 粘度調整剤(B)が、さらにポリオキシC2−4アルキレン基及び/又はアルキル基を有する請求項2記載のスクリーン印刷用導電性接着剤。
- 粘度調整剤(B)の割合が、金属ナノ粒子(A1)100質量部に対して1〜3質量部である請求項1〜3のいずれかに記載のスクリーン印刷用導電性接着剤。
- 保護コロイド(A2)の割合が、金属ナノ粒子(A1)100質量部に対して1〜3質量部である請求項1〜4のいずれかに記載のスクリーン印刷用導電性接着剤。
- 分散溶媒(C)が、大気圧下における沸点が220℃以上であり、かつ複数のヒドロキシル基を有する溶媒である請求項1〜5のいずれかに記載のスクリーン印刷用導電性接着剤。
- 第1の無機素材に請求項1〜6のいずれかに記載のスクリーン印刷用導電性接着剤をスクリーン印刷する印刷工程、第2の無機素材で前記導電性接着剤を挟み込んだ後、100℃以上で加熱して前記導電性接着剤を焼結する焼結工程を含む無機素材の接合体の製造方法。
- 第1及び第2の無機素材の少なくとも一方の接合面が貴金属を含む請求項7記載の製造方法。
- 請求項7又は8記載の製造方法により得られた無機素材の接合体。
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